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Nickel phosphide catalyst used for producing 2,3,3,3-tetrafluoropropene through gas-phase selective hydrodechlorination

A technology for selective hydrogenation and tetrafluoropropene, which is used in physical/chemical process catalysts, dehydrohalogenation preparation, organic chemistry, etc. It can solve the problems of reduced selectivity of target products and increased cost of reaction processes, and achieve high temperature sintering resistance. Good, low cost of raw materials

Active Publication Date: 2019-07-16
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the preparation methods disclosed in these several patents, although 1,1-dichloro-2,3,3,3-tetrafluoropropene or 1-chloro-2,3,3,3-tetrafluoropropene can be directly mixed with hydrogen One-step reaction to prepare 2,3,3,3-tetrafluoropropene, but in the actual reaction process, the double bond in the raw material compound will preferentially react with hydrogen to form saturated chlorofluoroalkanes, resulting in a decrease in the selectivity of the target product
At the same time, the active components of the catalyst used are all noble metals, and the reaction raw materials also need to be prepared through complicated steps, resulting in an increase in the cost of the entire reaction process

Method used

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  • Nickel phosphide catalyst used for producing 2,3,3,3-tetrafluoropropene through gas-phase selective hydrodechlorination

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: prepare Ni 2 P / oxide (fluoride, molecular sieve) catalyst

[0023] 9.48g nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) and 3.45g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 20 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear green solution. According to the loading of 0.5%, 5%, 10%, 20%, and 30%, the above solutions are impregnated onto a certain mass of oxides, fluorides, or molecular sieves, and then aged at room temperature for 12 hours, dried at 120 ° C for 12 hours to dry the water, and Calcined at 500°C for 3h to obtain the precursor of phosphate. The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and kept at 120°C for 1h to remove...

Embodiment 2

[0024] Embodiment 2: prepare Ni 12 P 5 / activated carbon catalyst

[0025] 9.48g nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) and 1.79g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 20 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear green solution. According to the loads of 5%, 10%, 20%, and 30%, the above solutions were impregnated on a certain mass of activated carbon, and then aged at room temperature for 12 hours, dried at 120 ° C for 12 h, and roasted at 500 ° C for 3 h in a nitrogen atmosphere to obtain Phosphate precursor. The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and kept at 120°C for 1h to remove the water adsorbed by the catalyst; (2) fro...

Embodiment 3

[0026] Example 3: Using the catalyst prepared by the method in Example 1 and 2, apply it to the gas phase selective hydrodechlorination of 2-chloro-1,1,1,2-tetrafluoropropane to prepare 2,3,3,3- In the reaction of tetrafluoropropene, after running for 8 hours, the reaction results are as follows:

[0027] Table 1 Conversion rate and product selectivity of HCFC-244bb on nickel phosphide catalysts with different loadings on different carriers for selective hydrodechlorination reaction.

[0028] Numbering catalyst HCFC-244bb conversion rate / % HFO-1234yf selectivity / % 1 0.5wt.%Ni 2 P / SiO 2

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Abstract

The invention discloses a nickel phosphide catalyst used for producing 2,3,3,3-tetrafluoropropene through selective hydrodechlorination. The nickel phosphide catalyst used for producing the 2,3,3,3-tetrafluoropropene through selective hydrodechlorination aims to solve the problems that by directly removing hydrogen chloride from 2-chloro-1,1,1,2-tetrafluoropropene to produce 2,3,3,3-tetrafluoropropene, reaction temperature is high, and catalyst inactivation is liable to happen. The catalyst is composed of a NixPy / carrier, wherein NixPy is a nickel phosphide covalent compound which is formed bycombining metal nickle and the non-metallic phosphorus and is of a crystal structure. The catalyst is excellent in performance, high in activity and good in stability, and reaction temperature is low, so that reaction energy consumption is effectively reduced, and the catalyst has industrial application values.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing 2,3,3,3-tetrafluoropropene by gas-phase selective hydrogenation dechlorination. It belongs to multiple catalytic technical fields. Background technique [0002] 2,3,3,3-tetrafluoropropene, referred to as HFO-1234yf, the molecular formula is CF 3 CF=CH 2 , non-toxic, non-flammable, ODP is zero, and GWP is about 4. It is considered to be an ideal substitute for HFC-134a and one of the most promising fourth-generation low-carbon refrigerants. [0003] So far, among the many known synthetic methods of HFO-1234yf, 1,1,2,3-tetrachloropropene and anhydrous hydrogen fluoride are mainly used as raw materials to synthesize the target product through a three-step reaction (Chinese patent CN102603465.A), The final step of the reaction is dehydrochlorination by 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) in the presence of a catalyst. Literature (ChemCatChem 2017, 9,824–832) and...

Claims

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Application Information

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IPC IPC(8): B01J27/185C07C17/25C07C21/18
CPCB01J27/1853C07C17/25C07C21/18
Inventor 田松吕剑白彦波贾兆华秦越马辉李晨王博毛伟
Owner XIAN MODERN CHEM RES INST
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